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本文研究了以5-Br-pADAP作显色剂,利用三阶导数光谱法,在碱性介质中同时测定铜和锌。该法测得铜、锌的表观三阶导数摩尔吸光系数分别为1.0×10 ̄5和3.0×10 ̄5,同时解决了谱带相互重叠干扰的问题。对石油化工厂污水进行测定,得到满意结果。 相似文献
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1-(2-苯并噻唑)-3-(4-硝基苯)-三氮烯的合成及其与镉(Ⅱ)的显色反应研究 总被引:6,自引:0,他引:6
报道了1-(2-苯并噻唑)-3-(4-硝基苯)-三氮烯(BTNPT)的合成及与镉(Ⅱ)的显色反应研究。在TritonX-100的存在下,pH11.6时,镉(Ⅱ)与BTNPT形成摩尔比=1∶2型黄色络合物,在435nm处有一最大正吸收,在530nm处有最大负吸收。以435nm为参比波长,530nm为测量波长进行双波长测定,表观摩尔吸光系数为2.52×105L·mol-1·cm-1,线性范围为0~10μg/25mL。已用于测定地面水和人发中的镉含量。 相似文献
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新试剂3,5—二溴—4—偶氮变色酸苯基荧光酮与锆(Ⅳ)显色反应的研究及应用 总被引:7,自引:3,他引:7
研究了在表面活性剂CTMAB存在下,新试剂3,5-二溴-4-偶氮变色酸苯基荧光酮与锆(Ⅳ)显色反应条件和光度性质。在0.5mol/L盐酸介质中,形成红色胶束配合物,最大吸收波长为539nm,表观摩尔吸光系数为1.74×105L·mol-1·cm-1,锆含量在每25mL0~10μg范围内服从比尔定律。拟定方法用于直接测定铝合金中微量锆,结果满意。 相似文献
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本文研究了新显色剂5'-硝基水杨基荧光酮(5'-NSF)在阳离子表面活性剂溴化十六烷基三甲铵(CTMAB)存在下与铬(Ⅵ)的显色反应。在pH5.5~6.7的磷酸盐缓冲介质中,Cr(Ⅵ)与5'-NSF反应生成组成比为1+4的水溶性和稳定性皆佳的紫色配合物,吸收峰波长λmax=586nm,对比度△λ=63nm,表观摩尔吸光系数586=1.74×105L·mol-1·cm-1,桑德尔灵敏度是3.0×10-4μg·cm-2,Cr(Ⅵ)浓度为0~0.21μg/mL时服从比尔定律。采用阴离子交换树脂分离,能够消除许多金属离子的干扰。方法用于水样中微量总铬、Cr(Ⅵ)和Cr(Ⅲ)的测定,结果较满意 相似文献
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新三氮烯类显色剂BBNDAB与铜(Ⅱ)显色反应的光度特性及其应用 总被引:1,自引:0,他引:1
本文报道了新显色剂3-溴-4(-2溴-4-硝基苯基重氮氨基)偶氮苯(BBNDAB)与铜(Ⅱ)的显色反应及分析应用。在TritonX-100存在下,于pH7.8的磷酸二氢钾-硼砂缓冲介质中,铜与该试剂形成配位比为1:2的红色配合物,最大吸收波长位于512nm,表观摩尔吸光系数为1.22×105L·mol-1·cm-1。反应有很好的选择性。不经分离、掩蔽可直接测定环境水样及人发样中微量铜。 相似文献
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运用卡尔曼滤波递推法,以2-(5-溴-2-吡啶偶氮)-5-二乙氨基苯酚(5-Br-PADAP)为显色剂,建立了同时测定锰,铁,铜,锌,镉析相光度法,在pH9.0硼酸-氢氧化钠介质中,胶束溶液在95℃加热1h,配合物被TritonX-100相完全富集,最大吸收峰分别为锰566nm,铁556nm,铜560nm锌562nm镉557nm,工作曲线范围除镉为0~8μg/5ml外,其余均为0~10μg/5ml 相似文献
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用溶胶-凝胶法以磷钼酸(MPA)的镍盐溶液水解钛酸四丁酯制备了NiPMo/TiO2催化剂.使用ICP、 XRD、 TG-DTA、 IR、 TPD-MS和微反应技术研究了催化剂的化学组成、热稳定性、化学吸附性质和催化反应性能.杂多钼酸盐与TiO2通过O2-在TiO2表面发生了键合.在623 K下,杂多阴离子仍保持原有的Keggin结构.CO2在Lewis酸位Ni(Ⅱ)和Lewis碱位Ni-O-Mo的桥氧协同作用下生成CO2卧式吸附态Ni(Ⅱ)←O-(CO)←(O--Ni).丙烯有多种吸附态在催化剂上吸附.在563 K、 1 MPa和空速1500 h-1的反应条件下,丙烯的摩尔转化率为3.2%,产物MAA选择性为95%. 相似文献
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Different approaches for the synthesis of 1-benzyloxypyrazin-2(1H)-one derivatives from simple amino acids have been investigated. A library of 33 precursors for the preparation of N-hydroxy pyrazinones was obtained in moderate to good yields. 相似文献
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Toward new camptothecins. Part 6: Synthesis of crucial ketones and their use in Friedländer reaction
Laurent Gavara Thomas Boisse Jean-Pierre Hénichart Adam Daïch Philippe Gautret 《Tetrahedron》2010,66(38):7544-5571
In the context of the preparation of camptothecin and luotonin A analogs, the synthesis of some key keto-precursors and their use in Friedländer condensation are described. This paper also focuses on the stability of these keto intermediates and emphasizes the major differences between indolizinones and pyrroloquinazolinones series. Noteworthy is also the report of some original structures isolated as by-products of some experiments. 相似文献
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The Langevin paramagnetic theory can’t describe the relation between magnetization of ferrofluids and applied magnetic field. The structuralization of ferrofluids, which is considered the main influence factor of the magnetization, is regarded. The part of magnetization works is deposited when the structure is forming. This action influences the magnetization of ferrofluids directly or indirectly. On the base of the “compressing” model, the Langevin function that usually describes the magnetization of ferrofluid is modified, and a well-fitted curve is obtained. An equation of the relation between the equivalent volume fraction after being “compressed” and the intensity of magnetic field is discovered, which approximately describes the process of magnetization. The relation between the approximate initial susceptibility and the volume fraction can be obtained from modified formula. 相似文献
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Rebecca J. Burton Mandy L. CrowtherNeal J. Fazakerley Shaun M. FilleryBarry M. Hayter Jason G. KettleCaroline A. McMillan Paula PerkinsPeter Robins Peter M. SmithEmma J. Williams Gail L. Wrigley 《Tetrahedron letters》2013
The highly regioselective Buchwald–Hartwig amination at C-2 of the cheap and readily accessible reagent, 2,4-dichloropyridine with a range of anilines and heterocyclic amines is described. This new methodology is robust and provides a facile access to 4-chloro-N-phenylpyridin-2-amines on 0.25 mol scale. These intermediates undergo a further Buchwald–Hartwig amination at higher temperature to enable rapid exploration of the chemical space at C-4 and to provide a library of 2,4-bisaminopyridines. 相似文献
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KMnO4-mediated oxidative CN bond cleavage of tertiary amines producing secondary amine was introduced, which was trapped by electrophiles (acyl chloride and sulfonyl chloride) to form amides and sulfonamides. The reaction could take place at mild condition, tolerating a wide range of function groups and affording products in moderate to excellent yields. 相似文献
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N. A. Nedolya 《Chemistry of Heterocyclic Compounds》2008,44(10):1165-1219
The review contains a concise historical account and information on the most significant researches undertaken by the staff
at the A. E. Favorsky Irkutsk Institute of Chemistry, Siberian Branch of the Russian Academy of Sciences on the Chemistry
of Heterocyclic Compounds.
Dedicated to Academician of the Russian Academy of Sciences B. A. Trofimov on his 70th jubilee.
Translated from Khimiya Geterotsiklicheskikh Soedinenii, No. 10, pp. 1443–1502, October, 2008. 相似文献
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A general synthesis of previously unknown semicarbazone-based α-amidoalkylating reagents, 4-(tosylmethyl)semicarbazones, has been developed. The synthesis involved three-component condensation of semicarbazones of aliphatic or aromatic aldehydes with the same or other aldehydes and p-toluenesulfinic acid. The scope and limitations of this reaction were investigated. The compounds obtained were demonstrated to be an efficient α-(4-semicarbazono)alkylating agents. They were reacted with H- (sodium borohydride), O- (sodium methylate), S- (sodium phenylthiolate), N- (pyrrolidine, sodium succinimide), P- (trialkyl phosphites), and C-nucleophiles (sodium diethyl malonate) to give the corresponding products of the tosyl group substitution, 4-substituted semicarbazones, including analogues of nitrofurazone. Among the prepared compounds tested in vitro for antibacterial and antifungal activity, three nitrofuryl-containing semicarbazones exhibited high biological activities with minimum inhibitory concentration (MIC) values of 8–32 μg/mL. 相似文献
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Regiospecific and direct imidation of the methyl C(sp3)–H bond of thioanisoles is realized under mild and metal-free conditions with N-fluorobis(benzenesulfonyl)imide as an oxidant and nitrogen source. Proposed mechanism suggests that thionium ion intermediates and a Pummerer-type reaction are involved. The imidation has advantages such as high step-economy, excellent functionality tolerance, and regiospecificity, giving structurally diverse imidation products. 相似文献
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A small library of new chiral bidentate hydroxyalkyl-imidazolium salts 1 is conveniently synthesized on multi-gram scale from inexpensive and commercially available chiral pool amino acids. The corresponding carbenes, generated by deprotonation of imidazolium salts 1, in combination with palladium(II) chloride were tested in the Mizoroki–Heck coupling reaction. The most significant results in terms of yields and reactivities were achieved with low catalyst loading. The catalytic activities of these imidazolium salts were also investigated in the asymmetric addition of diethylzinc to benzaldehyde. The use of MgO nanoparticles as an additive in conjunction with these ligands played a crucial role in increasing the efficiency of these reactions. 相似文献